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The use of matrix-specific calibrations for oxygen in analytical glow discharge spectrometry.

Gonzalez-Gago C, Smid P, Hofmann T, Venzago C, Hoffmann V, Gruner W - Anal Bioanal Chem (2014)

Bottom Line: The importance of a "blue shifted" line of oxygen at 130.22 nm (first reported by Köster) for quantitative analyses by GD-OES is confirmed.Matrix-specific calibrations for oxygen in GD-MS are presented.Additional experiments using Ar-He mixtures or μs pulsed GD are carried out in ELEMENT GD aiming to improve the oxygen sensitivity.

View Article: PubMed Central - PubMed

Affiliation: Leibniz Institute for Solid State and Materials Research (IFW) Dresden, P.O. Box 270116, 01171, Dresden, Germany.

ABSTRACT
The performance of glow discharge optical emission spectroscopy and mass spectrometry for oxygen determination is investigated using a set of new conductive samples containing oxygen in the percent range in three different matrices (Al, Mg, and Cu) prepared by a sintering process. The sputtering rate corrected calibrations obtained at standard conditions for the 4 mm anode (700 V, 20 mA) in GD-OES are matrix independent for Mg and Al but not for Cu. The importance of a "blue shifted" line of oxygen at 130.22 nm (first reported by Köster) for quantitative analyses by GD-OES is confirmed. Matrix-specific calibrations for oxygen in GD-MS are presented. Two source concepts-fast flow (ELEMENT GD) and low gas flow (VG9000)-are evaluated obtaining higher sensitivity with the static flow source. Additional experiments using Ar-He mixtures or μs pulsed GD are carried out in ELEMENT GD aiming to improve the oxygen sensitivity.

No MeSH data available.


Related in: MedlinePlus

Oxygen calibration (corrected by sputtering rates) in GD-OES. The samples were measured at standard conditions for the 4-mm dc source (700 V, 20 mA). The horizontal lines represent the intensities corresponding to the pure sintered samples (short dashed line for Al, dashed line for Cu, and dotted line for Mg)
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Fig3: Oxygen calibration (corrected by sputtering rates) in GD-OES. The samples were measured at standard conditions for the 4-mm dc source (700 V, 20 mA). The horizontal lines represent the intensities corresponding to the pure sintered samples (short dashed line for Al, dashed line for Cu, and dotted line for Mg)

Mentions: The resulting sputtering rate corrected calibration is shown in Fig. 3. Besides the data of the three matrices Cu, Al, and Mg this figure also includes the point of the well know highpoint calibration sample CE 650 from Jernkontoret (32.4 % m/m oxygen). This calibration material with higher concentration of oxygen is used to overcome the problems of the exact determination of the light element at low levels. The horizontal lines represent again the intensities of the pure sintered samples. Equally in Fig. 3, no error bars are shown. The relative error estimated based on several measurements is <10 %.Fig. 3


The use of matrix-specific calibrations for oxygen in analytical glow discharge spectrometry.

Gonzalez-Gago C, Smid P, Hofmann T, Venzago C, Hoffmann V, Gruner W - Anal Bioanal Chem (2014)

Oxygen calibration (corrected by sputtering rates) in GD-OES. The samples were measured at standard conditions for the 4-mm dc source (700 V, 20 mA). The horizontal lines represent the intensities corresponding to the pure sintered samples (short dashed line for Al, dashed line for Cu, and dotted line for Mg)
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4225055&req=5

Fig3: Oxygen calibration (corrected by sputtering rates) in GD-OES. The samples were measured at standard conditions for the 4-mm dc source (700 V, 20 mA). The horizontal lines represent the intensities corresponding to the pure sintered samples (short dashed line for Al, dashed line for Cu, and dotted line for Mg)
Mentions: The resulting sputtering rate corrected calibration is shown in Fig. 3. Besides the data of the three matrices Cu, Al, and Mg this figure also includes the point of the well know highpoint calibration sample CE 650 from Jernkontoret (32.4 % m/m oxygen). This calibration material with higher concentration of oxygen is used to overcome the problems of the exact determination of the light element at low levels. The horizontal lines represent again the intensities of the pure sintered samples. Equally in Fig. 3, no error bars are shown. The relative error estimated based on several measurements is <10 %.Fig. 3

Bottom Line: The importance of a "blue shifted" line of oxygen at 130.22 nm (first reported by Köster) for quantitative analyses by GD-OES is confirmed.Matrix-specific calibrations for oxygen in GD-MS are presented.Additional experiments using Ar-He mixtures or μs pulsed GD are carried out in ELEMENT GD aiming to improve the oxygen sensitivity.

View Article: PubMed Central - PubMed

Affiliation: Leibniz Institute for Solid State and Materials Research (IFW) Dresden, P.O. Box 270116, 01171, Dresden, Germany.

ABSTRACT
The performance of glow discharge optical emission spectroscopy and mass spectrometry for oxygen determination is investigated using a set of new conductive samples containing oxygen in the percent range in three different matrices (Al, Mg, and Cu) prepared by a sintering process. The sputtering rate corrected calibrations obtained at standard conditions for the 4 mm anode (700 V, 20 mA) in GD-OES are matrix independent for Mg and Al but not for Cu. The importance of a "blue shifted" line of oxygen at 130.22 nm (first reported by Köster) for quantitative analyses by GD-OES is confirmed. Matrix-specific calibrations for oxygen in GD-MS are presented. Two source concepts-fast flow (ELEMENT GD) and low gas flow (VG9000)-are evaluated obtaining higher sensitivity with the static flow source. Additional experiments using Ar-He mixtures or μs pulsed GD are carried out in ELEMENT GD aiming to improve the oxygen sensitivity.

No MeSH data available.


Related in: MedlinePlus